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Method for grafting environment response macromolecule on nano silicon dioxde surface

A technology of nano-silica and environmental responsiveness, which is applied in the field of synthesis and preparation of organic-inorganic hybrid materials. The method is simple and easy, and the effect of reunion does not occur

Inactive Publication Date: 2008-03-12
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Due to the small particle size, large specific surface area, and high surface energy of nano-silica, it is easy to agglomerate with each other and has poor compatibility with most polymer materials. It is difficult to obtain uniform dispersion at the nanoscale by using existing general technologies. To the purpose of particle nano-filling, it will affect the performance of the material

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] a. Add 3g of nano-silica, 60mL of dry toluene and 12mL of 3-aminopropyltrimethoxysilane in sequence, and pump argon gas into the reaction system three times to remove the water vapor in the system. Refluxing reaction in an oil bath for 36 hours, lowering the temperature and standing still, followed by ultrasonic washing with a large amount of toluene and acetone to remove the adsorbed silane reagent, centrifugal separation, and vacuum drying at room temperature for 24 hours to obtain nano-silica whose surface terminal group is amino group;

[0022] b. Add 0.3g of nano-silica connected to amino groups, 20mL of dry toluene and 8mL of dry triethylamine in a dry flask, put 4mL of 2-bromopropionyl bromide and 8mL of dry toluene in an ice-water bath with a dropping funnel Slowly drop the mixed solution of the three-necked flask into the three-necked flask, react for 4 hours, let it stand for precipitation, sequentially use a large amount of toluene and acetone / water as the sol...

Embodiment 2

[0026] a. Add 1g of nano-silica, 20mL of dry toluene and 4mL of 3-aminopropyltrimethoxysilane in sequence, and pump argon gas into the reaction system three times to remove the water vapor in the system. Reflux reaction in an oil bath for 12 hours, lower the temperature and let it stand, sequentially wash with a large amount of toluene and acetone to remove the adsorbed silane reagent, centrifuge, and vacuum dry at room temperature for 24 hours to obtain nano-silica whose surface terminal group is amino;

[0027] b. Add 0.6g of nano-silica connected to amino groups, 40mL of dry toluene and 16mL of dry triethylamine in a dry flask, put 8mL of 2-bromopropionyl bromide and 16mL of dry toluene in an ice-water bath with a dropping funnel Slowly drop the mixed solution into the three-necked flask, react for 24 hours, let stand to precipitate, sequentially use a large amount of toluene and acetone / water as solvents to ultrasonically wash, centrifuge, and vacuum dry at room temperature...

Embodiment 3

[0031] a and b steps are the same as in Example 1.

[0032] c. In the flask, add 0.1g of nano-silica with ATRP initiator group at the end, THF 1mL, monomer DMAEMA 0.01mol, CuBr 0.019g and PMDETA 27uL, and the reactor is pumped with Ar three times under liquid nitrogen cooling. Under the protection of Ar, react in an oil bath at 65°C for 48 hours, let it stand for cooling, wash the precipitate with THF and acetone in sequence, centrifuge, and dry it in vacuum at room temperature for 2 hours to obtain a silica / dimethylaminoethyl methacrylate core-shell Structural Nanohybrid Particles.

[0033] The hybrid nanoparticles prepared by the method have a grafting rate of 70.5%, no agglomeration phenomenon, and good dispersibility and pH-temperature responsiveness.

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PUM

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Abstract

The present invention relates to a preparation method for organic-inorganic hybrid materials through grafting polymerization-environment responsive macromolecules on the nanometer silicon dioxide surface, belonging to the organic-inorganic hybrid materials synthesis and preparation field. The present invention takes advantage of the action of silicon dioxide with hydroxyl on the surface with the silane coupling agent 3-amino-propyl silane to enable the end to be of an amino group; then the product reacts with the nanometer particle generated from the bromination propionyl bromine reaction; The end of the nanometer particle is the ATRP initiator; finally, the polymerization of the environmentally-responsive macromolecules on the nanometer silicon dioxide surface is initiated in the present of CuBr and PMDETA so as to obtain the target product. The graft rate of the silicon dioxide virgule environmentally-responsive macromolecule core-shell structure nanometer hybrid particles is 60 percent to 70 percent. No reunion of the nanometer hybrid particles appears. The nanometer hybrid particles are uniformly dispersed with environmental responsiveness.

Description

technical field [0001] The invention relates to a method for grafting and polymerizing environment-responsive macromolecules on the surface of nano silicon dioxide to prepare organic-inorganic hybrid materials, and belongs to the field of synthesis and preparation of organic-inorganic hybrid materials. Background technique [0002] With the development of science and technology, nano-organic / inorganic hybridization of functional materials is the trend of modern material development. New functional materials can be prepared by hybridizing two or more organic / inorganic chemical components to complement and optimize their properties. Nano-organic / inorganic hybrid materials combine the excellent properties of organic polymers, inorganic materials and nano-materials, have diverse structures and unique physical and chemical properties, and open up a new way for people to explore new materials. [0003] Nano-silica and environment-responsive polymers can be synthesized to obtain i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F292/00C08K3/36
Inventor 袁金颖周莅霖袁伟忠周密隋晓锋
Owner TSINGHUA UNIV
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